Maturing process and apparatus therefor.



J. E. CARROLL. MATURING PROCESS AND APPARATUS THEREFOR.

Patented Aug. 30, 1910.

2 SHEETS-SHEET 1.

v 'nwnfoz nzmesil' JarmZZ 6 m may/6;

APPLIQATIDI FILED NOV. 7, 1908.

llvilimmmw J'. E. CARROLL. MATURING PROCESS AND APPARATUS THEREFOR.-

APPLIUATION IILBD NOV. 7, 1908.

Patented Aug. 30, 1910.

2 SHEETS-SHEET 2.

'To all whom it may concern: I

prises a method of maturing or low 7 JAMES EDMU.ND CARROLL, OF LONDON,ENG-IiAND.

MATURING- PROCESS AND APPARATUS THEREFOR.

Specification of Letters Patent.

Application filed November 7, 1908. Serial 1:... 461,578.

Be it known-that I, JAMES EDMUND CAR- ROLL, a citizen of the UnitedStates, residing at London, England, have invented certain new anduseful Improvements in Maturing Processes and Apparatus Therefor, ofwhich the following is a specification.

This invention relates to maturing processes and apparatus therefor; andit com- 77 whisky and similar distilled spirits wherein alcoholic vaporscoming from a still, and preferably in a certain stage of the distillaetion, are commingled with heated air and exposed to the action of heatunder repeated commingling and under effective contact withcatalytically-acting hot metallic walls; and it also comprises anapparatus for maturing and aging distilled spirits which comprises meansfor producing distilled alcoholic vapors, means for mixing air with saidvapors, means for repeatedly mingling said air and vapors, and means forexposing the mixture to the action of heated catalytically-acting wallsand in intimate contact with such walls, all portions of such mixturecoming into contact with such walls; all as more fully hereinaftersetforth and as claimed.

In the usual methods of making whisky,

rum and other distilled liquors, the distillate from the fermented mashis ordinarily stored for a long period of time, usually a.

number of years, in order to mature or age it. The storage is usuall inoaken barrels.

During the storage, the iquor undergoes a number of changes of obscurenature which result in rendering it palatable and potable whereas thecrude condensate from the stills is hardly drinkable, having a harsh,new flavor. Whisky aged in wood has :1 inclflavor. While the --nature ofthe changes is, as stated, obscure, they are apparently due in some wayto oxidation, air

penetrating more or less into the barrels in which the aging or maturingis done, and in some manner developing taste and aroma producing ethersor esters, or, probably, both.

In the prior art many methods of performing a quick oxidation have beenat tempted; this being generally done by aerating the liquor duringstorage. Such aeratmg processes however, in spite of their closeimitation of the natural maturing processes, have hardly provedsatisfactory 1n giving the desired results within any reasonable time,oxidation at comparatively low temperatures, such as must of course beused with alcoholic liquids, being a slow operation and also somewhatuncertain, since the taste and aroma produced in this way are not alwaysof the most desirable type. In a prior process, (Patent N 0. 666,242) Ihave departed from this method of maturing by aerating the heated vaporsin lieu of the condensed liquid and have thereby secured much moreuniform, speedy and desirable results. In the present process I havestill further improved this method the nature and extent of the reactionbetween the air and the-vapors by controlling certain conditions. I havediscovered that the said reaction is not merely a matter of heat alonebut is, like other chemical reactions,-much aflected by the nature ofthe vessels in which it is performed and particularly by what is knownas wall action; and that by bringing the mixture of air" and vapors intovery intimate and thorough contact with catalytically acting heatedmetal walls while preserving a definite range of temperatures, a highlydesirable type of action takes place, giving matured liquors ofexceptional mellowness. This contact of the air-Vapor mixture with thewall surface must be positive in its nature, every portion of suchmixture coming into such contact. In any large body of mixed air andalcohol vapor it is, however,-very diflicult to secure such an intimatecontact of every particle of such body with the walls, to the difficultyin overcoming stratification in such a heterogeneous mixture if of anylarge volume and partly to the sheer difli-' culty. of securingcirculation. The specific gravity of alcohol vapor and air diflers veryPatented Aug. 30, 1910.

owing partly widely. These difliculties increase more thanproportionately with an increase in volume, and they persist even wherethe body of gas is converted into a flowin current, as in alarge-diameter pipe; an particularly where the pipe is heated, since theheating tends to preserve the Stratification. Practically, it may besaid that with any flowing current of gas or vapor over an inch or so indiameter, it is -difiieult to insure any perfect mixture so that everyportion of the current of such mixture shall come into actual contactwith the materials of the conduit wall in any reasonable length oftravel.

In catalyzing a mixture of spirit vapor and air, such perfect mixtureand actual contact are, however, as I find, imperatively necessary forthe best results. Any portion of the air-vapor mixture which has notcome into contact with the conduit walls, even if heated to whatevertemperature is employed in maturing, is apt to be insufficiently maturedand upon condensation and admixture with the rest of the maturedmaterial will depreciate its quality.

In the present invention, therefore, I take the stream of vapor flowingfrom the head of an ordinary ot-still, admix it with air and thensubdivide the mixture into a plurality of relatively small streams, eachof comparatively small diameter, and ass these streams through separateheated pipes, each of corresponding diameter. And still further toreduce the danger of Stratification which might lead these streams,drawn from a body of mixed air and vapor, to be of differentcomposition, I preferably use the air in a heated state. Cold air andheated vapor are difficult to mix uniformly while hot air mixes well.And with heated air, the heating duty of the heated conduits is ofcourse reduced. Furthermore, after the separate streams have traveledthrough their respective heated conduits for a time,

I preferably remix them and again 'subdivide into separate streams. Suchre-commingling from time to time is very advantageous. In the presentprocess it is desirable that every molecule, so to speak, of the vaporshall have a molecule of oxygen lying next it and that these adjacentmolecules shall at some time in their travel through the apparatus comeinto contact with a heated metallic wall. In securing this commingling,it is desirable that the direction of flow through the conduits bereversed at each commingling. If a two-stratum layer of gas travelthrough a conduit to the right, emerge into an end chamber and thencetravel through another conduit to the left, the upper and lower stratatend to be reversed; an effect which much promotes commingling.

The metal of the conduits used. in the present invention is preferablycopper as it combines a good resistance against the action of theair-vapor mixture with an efficient cataly'zing action for the presentpurposes.

The temperature employed in the catalyzing1 operation is of considerableimportance. W ile there is a certain range of temperatures for eachparticular distilled liquor, a temperature of about 300 F. is welladapted for most. In manufacturing Scotch whisky, for example, anaverage temperature 7 of about 300'F. is quite suitable. The temperatureshould not fall below 280 F. or rise above 320. Below the firsttemperature, the maturing action is slow and ineifi cient; above thelatter temperature the characteristic malt fiavdr of the whisky tends todisappear.

It is further desirable in the present process that the whole body ofvapors be not sent through the maturing apparatus, but that 7 both theforerunnings and the after runnings be by-pressed around it, leavingmerely the intermediate portion to be treated. With both thesefractions, oxidation under the described conditions is apt to 5 be tooactive. v

In the accompanying illustration, I have shown, more or lessdiagrammatically, certain embodiments of apparatus elements useful inperforming the described process and in other relations.

In this showing Figure 1 is a view in elevation showing, more or lessdiagrammatically, an ordinary pot still and condenser and maturingapparatus connected therewith 5 Fig. '2 is a view of the maturingapparatus, partly broken away; Fig. 3 is a detail view showing thereversal of vapor strata in reversing' the direction of flow; and Fig. 4is a View showing the maturing apparatus in 0 connection with a columnstill.

In Fig. 1, element 1 is an ordinary pot still, provided with the usualhead 2. From the head, conduit 3 leads vapor away .to a condenser (shownas an ordinary worm condenser) 4. In the vapor conduit is a valve,

5, and tapping the conduit on either side of this valve are two vaporlines, 6 and 7,

' valved respectively at 8 and 9. The vapor line nearer the still leadsvapors to the maoo turing apparatus proper while the other returns thetreated vapor to the vapor conduit.

Vapor line 6, as shown, leads downward to the mixing chamber 10.Entering this chamber is an air pipe 11, ending in a rose or otherdistributer, 12, therewithin, and valved at 13. This air pipederivesheated air from heater 14, shown as a simple casing having steam inlet15 and outlet 16, containing a helical air pipe 17, supplied by-lio pipe18 from a fan or blower (not shown). The mixture of air and vapor istreated in a'series of superheaters (five are shown), letteredrespectively A, B, C, D and E, and like in structure. Each superheatercontains a nest of tubes, 19, preferably not over an inch in diameter,contained in a heating casing, 20, provided with a cross-header at eachend, respectively 21 and 22. These headers form mixing chambers ateither end with an intermediate steam chamber, 23. The mixing chamber atthe entrance end of the lowermost casing has already been described. Themixture of vapor and heated air in this chamber is sub-divided into asmany small streams as there are tubes and the streams from these tubesare again intermingled at the mixing chamber 24 at the other end of thesuperheater. This latter chamber is provided with an uptake 25 connectedwith the mixing chamber 26 next in series, and so on throughout theseries. The mixing chamber 27 at the exit end of the uppermostsuperheater (A) with the return Vapor line (7).

The steam chambers of the various superheaters are fed by steam-line 28and ex hausted by. outlet line 29. As shown, 29 supplies exhaust steamfor the air heater. Each superheater is provided with a petcock, 30, forremoving entrapped air or gas. The apparatus is further provided withsafety valve 31, pressure gage 32, thermometer 33 in the return vaporline, and pyrometer 34 in the steam line.

In Fig. 3, which is a mere diagrammatic view to show reversal of vaporstrata, strata o and p leaving a pipe 35 and flowing upward through anend chamber 36 and thence backward through another pipe 37, tend toreverse in position as shown. In the actual apparatus of Figs. 1 and 2,which have a plurality of tubes, the mixing action is much Y morecomplicated, but this view shows it in denser.

a simplified form.

In Fig. 4, 38 shows, diagrammatically, a broken away section of anordinary column still, interrupted by a transverse partition 39. Abovethis partition, enters pipe 40 re turning vapors from diagrammaticallyshown. superheater 41 while below it pipe 42 abstracts alcohol vaporsand delivers the same to said superheater. The column still is,preferably, a rectifying column, such as is used with the ordinary typesof Coffey still. When used as such, concentrated, purified alcohol maybe removed from the apparatus above the diaphragm by pipe 43. Anordinary heat-interchanger 44 may be interposed in the communicationbetween still and superheater to insure return of the superheatedvaporsto the still at still tem perature.

The operation of the devicesshown is apparent from the foregoing. InFigs. 1 and 2, valve 5 may be opened while the first portion ofdistillate is coming from the still, valves 8 and 9 being closed, andthis distillate is thereby by-passed around the maturing apparatus anddelivered to the con- WVhen tolerably pure alcoholic vapor appears, thevalve 5 is closed and 8 and 9 opened, whereby the alcoholic vapors areled through the maturing device. The alcoholic vapors are admixed-withheated air in 10 and the mixture passes onward as a plurality ofrelatively narrow streams through the several tubes of the. tube nest,being heated by the steam in the steam chamber. The mixture, for Scotchwhisky, is preferably kept at a temperature around 300 F. Steam of 500to 700 F.,'expanded to only 7 or 8 pounds pressure, may be used in theheating jacket. The mixture of air and vapor being passed through thesenarrow is connected tubes substantially all portions of the mixture comeinto actual contact with the tube walls. Emerging from the first tubenest, the mixture passes into the mixing chamber at the other end of thesuperheater and is thoroughly commingled therein, the reversing tendencyof the change of direction of flow materially aiding in thiscommingling. The mixed body in this mixing chamber is again subdividedinto a plurality of narrow streams in the second superheater (D) and soon through the series. IVhen the alcoholic vapors coming from the stillbecome less pure, it is preferable to by-pass them around .thesuperheater, thus confining the maturing action to the purer midportionof'the distillate.

In using the apparatus of Fig. 4, '38 is preferably a rectifying still,separating fusel oil and aldehyde from the alcohol so that the vaporstaken to the maturer by 42 and returned by 40 are substantially purealcohol. In another and co-pending application Ser. No. 469,3l8, filedDec. 26, 1908, I have described more specifically an apparatus of thistype and have claimed such apparatus and a process of improving thequality of concentrated alcohol vapors wherein such apparatus isemployed.

If preferred, the aeration in the maturing apparatus may be done at aplurality of points. Valved connection 50 permits air in regulatedamount to be supplied to any of the mixing chambers.

In the manufacture of Scotch whisky by the described process, thedistillate coming from the condenser has the taste, odor and chemicalcharacteristics of whisky which has been matured for a long time in woodand is devoid of the ordinary harsh, new flavor of new whisky. Similar,advantages are attained in the case of other distilled liquors.Distilled liquors so produced may be sent into the market directly anddo not require maturing, being, as a matter of fact, indistinguishablein most cases from spirits which have matured for several years wherethe operation has been conducted with the precautions previouslydescribed.

What I claim is 1. The process of preparing a matured potable liquorwhich comprises producing alcoholic vapors in a pot still, admixing thevapors from the still with heated air to form a mixed body, subdividingthe mixture into a plurality of relatively narrow streams and passingsuch streams past and in substantial contact with heated met-a1 walls,said streams being remingled at a plurality of points in their courseand condensing the treated vapors to form amatured potable liquor.

2. The process of preparing a matured potable liquor which comprisesproducing alcoholic vapors in a pot still, admixing the vapors from thestill with air to form a 3. The process of preparing a matured. potableliquor which comprises producing alcoholic vapors in a pot still,admixing the vapors from the still with air to form a mixed body,subdividing this body to form a plurality of relatively narrow streamsand passing such streams past and in substantial contact with heatedmetal walls, remingling the streams to form another united body,resubdividing into narrow streams and once more passing such streamspast and in substantial contact with heated metal walls and condensingthe't-reated vapors to form a matured potable liquor.. I

I 4. The process of treating alcoholic vapors which comprises mixingalcoholic vapors with heated air and transmitting said admixed vaporsand air as a relatively narrow stream through a metal conduit maintainedat a temperature" of about 300 F., no portion of said stream being morethan half an inch from a heated metal wall.

5. In the treatment of alcoholic vapors, the process which comprisesproducing alcoholic vapors in a still relatively free from higher andlower boiling spirituous impurities, admixing the vapors coming from thestill with air to produce a mixed body, subdividing this body into apluralitywof relatively narrow streams and passing such streams past andin substantial contact with heated metal walls, remingling the streamsto form another mixed body and once more subdividin such mixed body intoa plurality of relatively narrow streams and passing such streams pastand in substantial contact with heated metal walls.

6; In a maturing apparatus, a pot still serving as a source of alcoholicvapors, means for admixing such vapors with heated air to form'a mixedbody, and means for transcase in the Patent Office.

[SEAL] Correction in Letters Patent No. 968,832.

mitting'such mixed body in a plurality of relatively, narrow streamspast and in substantial contact with heated metal walls, means forremingling said streams and means for condensing the vapors treated.

7. In a maturing apparatus, the combina-.

tion with a. still serving as a source of alcoh'olic vapors of amaturing apparatus comprising means for mixing such vapors, with heatedair to form a mixed body, meansfor subdividing such mixed body into aplurality of relatively narrow streams and transmitting such streamspast and in sub stantial contact with heated metal walls, means forreuniting the several streams and commingling them, and means for oncemore subdividing them into relatively narrow streams and transmittingthem past and in substantial contact with heatedmetal'walls.

8. The process of producing a matured 9. The process of maturing vapors,which comprises admixing the comparatively large Volume stream of vaporscoming from an ordinary alcohol still with heated air, sub dividing suchadmixed stream into a plurality of relatively narrow streams and passingeach such narrow stream past and in substantial contact with heatedmetal walls, said streams being positively 'remingled and againsubdivided at a plurality of points in their course.

In testimony whereof I affix my signature, in

presence of two 'witnesses.

JAMES EDMUND CARROLL.

Witnesses:

JOHN H. SIGGERS, LEWIS EBERLY.

. It is hereby certifiedthat in Letters Patent No. 968,832, grantedAugust 30, 1910, upon the application of James Edmund Carroll, ofLondon, England, for an improvement in lllaturing Processes andApparatus Therefor, an error appears in the printed specificationrequiring correction as follows: Page 2, line 7 2, the compound wordby-pressed should read by-passerl; and that the said Letters Patentshould be read with this correction therein that the same may conform tothe record of the Signed and sealed this 27th day of September, A. ll,1910.

c. c. BILLINGS,

Act-mg Commissioner of Patents.

3. The process of preparing a matured. potable liquor which comprisesproducing alcoholic vapors in a pot still, admixing the vapors from thestill with air to form a mixed body, subdividing this body to form aplurality of relatively narrow streams and passing such streams past andin substantial contact with heated metal walls, remingling the streamsto form another united body, resubdividing into narrow streams and oncemore passing such streams past and in substantial contact with heatedmetal walls and condensing the't-reated vapors to form a matured potableliquor.. I

I 4. The process of treating alcoholic vapors which comprises mixingalcoholic vapors with heated air and transmitting said admixed vaporsand air as a relatively narrow stream through a metal conduit maintainedat a temperature" of about 300 F., no portion of said stream being morethan half an inch from a heated metal wall.

5. In the treatment of alcoholic vapors, the process which comprisesproducing alcoholic vapors in a still relatively free from higher andlower boiling spirituous impurities, admixing the vapors coming from thestill with air to produce a mixed body, subdividing this body into apluralitywof relatively narrow streams and passing such streams past andin substantial contact with heated metal walls, remingling the streamsto form another mixed body and once more subdividin such mixed body intoa plurality of relatively narrow streams and passing such streams pastand in substantial contact with heated metal walls.

6; In a maturing apparatus, a pot still serving as a source of alcoholicvapors, means for admixing such vapors with heated air to form'a mixedbody, and means for transcase in the Patent Office.

[SEAL] Correction in Letters Patent No. 968,832.

mitting'such mixed body in a plurality of relatively, narrow streamspast and in substantial contact with heated metal walls, means forremingling said streams and means for condensing the vapors treated.

7. In a maturing apparatus, the combina-.

tion with a. still serving as a source of alcoh'olic vapors of amaturing apparatus comprising means for mixing such vapors, with heatedair to form a mixed body, meansfor subdividing such mixed body into aplurality of relatively narrow streams and transmitting such streamspast and in sub stantial contact with heated metal walls, means forreuniting the several streams and commingling them, and means for oncemore subdividing them into relatively narrow streams and transmittingthem past and in substantial contact with heatedmetal'walls.

8. The process of producing a matured 9. The process of maturing vapors,which comprises admixing the comparatively large Volume stream of vaporscoming from an ordinary alcohol still with heated air, sub dividing suchadmixed stream into a plurality of relatively narrow streams and passingeach such narrow stream past and in substantial contact with heatedmetal walls, said streams being positively 'remingled and againsubdivided at a plurality of points in their course.

In testimony whereof I affix my signature, in

presence of two 'witnesses.

JAMES EDMUND CARROLL.

Witnesses:

JOHN H. SIGGERS, LEWIS EBERLY.

. It is hereby certifiedthat in Letters Patent No. 968,832, grantedAugust 30, 1910, upon the application of James Edmund Carroll, ofLondon, England, for an improvement in lllaturing Processes andApparatus Therefor, an error appears in the printed specificationrequiring correction as follows: Page 2, line 7 2, the compound wordby-pressed should read by-passerl; and that the said Letters Patentshould be read with this correction therein that the same may conform tothe record of the Signed and sealed this 27th day of September, A. ll,1910.

c. c. BILLINGS,

Act-mg Commissioner of Patents.

Correction in Letters Patent No. 968,832.

It is hereby certified that in Letters Patent No. 968,832, grantedAugust 30, 191 upon the application of James Edmund Carroll, of London,England, for an improv ment in Maturing Processes and ApparatusTherefor, an error appears in t1 printed specification requiringcorreetien as follows: Page 2, line 72, the eompoun Word by-preesedshould readby-pzwsed; and that the said Letters Patent shou] be readwith this correction therein that the same may conform to the record ofth case in the Patent Oflfice.

Signed and sealed this 27th day of September, A. D., 1910.

C. C. BILLINGS,

'[SEAL.]

Acting Commissioner of Patents.

